#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:45:22 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179392 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/89/4328986.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4328986
loop_
_publ_author_name
'Wen-Yang Gao'
'Wuming Yan'
'Rong Cai'
'Le Meng'
'Andrea Salas'
'Xi-Sen Wang'
'Lukasz Wojtas'
'Xiaodong Shi'
'Shengqian Ma'
_publ_section_title
;
 Porous Double-Walled Metal Triazolate Framework Based upon a Bifunctional
 Ligand and a Pentanuclear Zinc Cluster Exhibiting Selective CO2 Uptake
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4423
_journal_page_last               4425
_journal_paper_doi               10.1021/ic3002256
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C45 H25 N15 O12 Zn5'
_chemical_formula_weight         1294.65
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           108
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I 4 -2c'
_symmetry_space_group_name_H-M   'I 4 c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   28.368(3)
_cell_length_b                   28.368(3)
_cell_length_c                   33.958(4)
_cell_measurement_temperature    100(2)
_cell_volume                     27327(5)
_computing_cell_refinement       'APEX2 (Bruker, 2010); SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2010)'
_computing_data_reduction        'SAINT (Bruker, 2009);XPREP(Sheldrick,2008)'
_computing_publication_material  'APEX2 (Bruker, 2010)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'BRUKER SMART APEXII CCD'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.0910
_diffrn_reflns_av_sigmaI/netI    0.0403
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            72267
_diffrn_reflns_theta_full        10.82
_diffrn_reflns_theta_max         10.82
_diffrn_reflns_theta_min         0.83
_exptl_absorpt_coefficient_mu    0.187
_exptl_absorpt_correction_T_max  0.9907
_exptl_absorpt_correction_T_min  0.9815
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; (Sheldrick, 2003)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.629
_exptl_crystal_description       block
_exptl_crystal_F_000             5168
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
;
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.58(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         5595
_refine_ls_number_restraints     333
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0900P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1422
_refine_ls_wR_factor_ref         0.1502
_reflns_number_gt                4220
_reflns_number_total             5595
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3002256_si_002.cif
_cod_data_source_block           MTAF-1
_cod_original_cell_volume        27328(5)
_cod_database_code               4328986
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, z+1/2'
'-x, -y, z'
'x, -y, z+1/2'
'-y, -x, z+1/2'
'y, -x, z'
'-y, x, z'
'y, x, z+1/2'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1'
'-y+1/2, -x+1/2, z+1'
'y+1/2, -x+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, x+1/2, z+1'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Zn1 Zn 0.75315(5) 0.25315(5) 0.23964(9) 0.0864(5) Uani 1 2 d S
Zn2 Zn 0.83482(4) 0.25312(4) 0.16479(6) 0.0952(5) Uani 1 1 d .
Zn3 Zn 0.75271(4) 0.17235(4) 0.31354(6) 0.0957(5) Uani 1 1 d .
O30 O 0.7970(3) 0.2970(3) 0.1966(3) 0.106(3) Uani 1 2 d S
N2 N 0.7957(3) -0.1876(3) 0.3010(3) 0.089(2) Uani 1 1 d D
N3 N 0.8023(3) -0.1442(4) 0.3160(3) 0.092(2) Uani 1 1 d D
N1 N 0.7610(3) -0.1871(3) 0.2738(2) 0.073(2) Uani 1 1 d D
C48 C 0.7970(4) -0.0425(4) 0.3336(3) 0.141(3) Uani 1 1 d DU
H48 H 0.8181 -0.0602 0.3496 0.169 Uiso 1 1 calc R
C2 C 0.7720(4) -0.1157(4) 0.2983(3) 0.091(3) Uani 1 1 d DU
C5 C 0.7951(4) 0.0055(4) 0.3374(3) 0.145(4) Uani 1 1 d DU
H5 H 0.8149 0.0214 0.3557 0.174 Uiso 1 1 calc R
C1 C 0.7444(3) -0.1414(4) 0.2701(3) 0.093(3) Uani 1 1 d D
H1 H 0.7205 -0.1298 0.2531 0.111 Uiso 1 1 calc R
C4 C 0.7683(4) -0.0659(3) 0.3066(3) 0.121(3) Uani 1 1 d DU
O28 O 0.7883(3) -0.0991(4) 0.1320(3) 0.164(3) Uani 1 1 d D
O10 O 0.7899(4) 0.1027(3) 0.3389(3) 0.179(4) Uani 1 1 d DU
C58 C 0.7642(4) 0.0301(3) 0.3143(3) 0.155(4) Uani 1 1 d DU
C56 C 0.7619(5) -0.0765(4) 0.1573(4) 0.138(3) Uani 1 1 d DU
C55 C 0.7999(4) 0.0008(4) 0.1474(3) 0.170(4) Uani 1 1 d DU
H55 H 0.8250 -0.0151 0.1345 0.204 Uiso 1 1 calc R
C7 C 0.7384(4) -0.0409(4) 0.2822(4) 0.156(4) Uani 1 1 d DU
H7 H 0.7193 -0.0564 0.2632 0.187 Uiso 1 1 calc R
O29 O 0.7373(3) -0.1010(3) 0.1761(3) 0.141(3) Uani 1 1 d DU
C24 C 0.8006(4) 0.0489(4) 0.1521(3) 0.164(4) Uani 1 1 d DU
H24 H 0.8269 0.0661 0.1424 0.196 Uiso 1 1 calc R
C25 C 0.7621(4) -0.0237(3) 0.1617(3) 0.124(3) Uani 1 1 d DU
C6 C 0.7373(5) 0.0076(4) 0.2864(4) 0.175(4) Uani 1 1 d DU
H6 H 0.7174 0.0257 0.2697 0.210 Uiso 1 1 calc R
C9 C 0.7605(5) 0.0830(4) 0.3175(4) 0.167(4) Uani 1 1 d DU
C21 C 0.8065(4) 0.1524(4) 0.1588(3) 0.101(3) Uani 1 1 d DU
H21 H 0.8261 0.1450 0.1370 0.122 Uiso 1 1 calc R
C23 C 0.7645(4) 0.0729(3) 0.1704(3) 0.136(3) Uani 1 1 d DU
N19 N 0.8039(3) 0.1940(3) 0.1767(3) 0.107(3) Uani 1 1 d DU
C22 C 0.7747(4) 0.1210(3) 0.1781(3) 0.095(3) Uani 1 1 d DU
C26 C 0.7246(4) -0.0019(4) 0.1800(3) 0.154(3) Uani 1 1 d DU
H26 H 0.6984 -0.0195 0.1893 0.185 Uiso 1 1 calc R
O54 O 0.7317(4) 0.1029(3) 0.3001(3) 0.171(4) Uani 1 1 d DU
C57 C 0.7265(4) 0.0467(4) 0.1842(3) 0.160(4) Uani 1 1 d DU
H57 H 0.7011 0.0625 0.1969 0.192 Uiso 1 1 calc R
N20 N 0.7702(3) 0.1926(3) 0.2027(3) 0.094(2) Uani 1 1 d DU
N18 N 0.7538(3) 0.1492(3) 0.2049(3) 0.102(2) Uani 1 1 d DU
C12 C 0.7925(4) 0.2925(4) 0.0924(4) 0.119(3) Uani 1 2 d SDU
O11 O 0.8178(3) 0.2670(3) 0.1109(2) 0.138(3) Uani 1 1 d DU
C13 C 0.7923(3) 0.2923(3) 0.0490(4) 0.101(3) Uani 1 2 d SDU
N47 N 0.8083(3) 0.2743(3) -0.1354(3) 0.143(3) Uani 1 1 d DU
C16 C 0.7928(3) 0.2928(3) -0.0760(4) 0.131(3) Uani 1 2 d SDU
C47 C 0.7911(3) 0.2911(3) -0.0326(4) 0.153(4) Uani 1 2 d SDU
C14 C 0.8220(3) 0.2621(3) 0.0292(3) 0.142(3) Uani 1 1 d DU
H14 H 0.8427 0.2418 0.0432 0.170 Uiso 1 1 calc R
C54 C 0.8197(3) 0.2648(3) -0.0993(3) 0.144(3) Uani 0.50 1 d PDU
H54 H 0.8425 0.2425 -0.0908 0.173 Uiso 0.50 1 calc PR
N54 N 0.8197(3) 0.2648(3) -0.0993(3) 0.144(3) Uani 0.50 1 d PU
C15 C 0.8211(3) 0.2620(3) -0.0113(3) 0.134(3) Uani 1 1 d DU
H15 H 0.8416 0.2414 -0.0252 0.161 Uiso 1 1 calc R
O31 O 0.7104(2) 0.2104(2) 0.2792(3) 0.083(3) Uani 1 2 d S
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0005 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0017 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2605 0.5370 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N1 Zn1 N1 90.2(4) 6_665 10_654
N1 Zn1 O31 90.2(3) 6_665 .
N1 Zn1 O31 90.2(3) 10_654 .
N1 Zn1 N20 177.5(4) 6_665 16_544
N1 Zn1 N20 89.3(2) 10_654 16_544
O31 Zn1 N20 92.2(3) . 16_544
N1 Zn1 N20 89.3(2) 6_665 .
N1 Zn1 N20 177.5(4) 10_654 .
O31 Zn1 N20 92.2(3) . .
N20 Zn1 N20 91.1(5) 16_544 .
N1 Zn1 O30 91.0(3) 6_665 .
N1 Zn1 O30 91.0(3) 10_654 .
O31 Zn1 O30 178.3(4) . .
N20 Zn1 O30 86.6(3) 16_544 .
N20 Zn1 O30 86.6(3) . .
O29 Zn2 O11 114.0(4) 6_665 .
O29 Zn2 N19 121.4(4) 6_665 .
O11 Zn2 N19 105.2(4) . .
O29 Zn2 O30 108.9(4) 6_665 .
O11 Zn2 O30 104.7(4) . .
N19 Zn2 O30 100.8(4) . .
O29 Zn2 O28 55.1(3) 6_665 6_665
O11 Zn2 O28 82.0(3) . 6_665
N19 Zn2 O28 91.5(4) . 6_665
O30 Zn2 O28 163.7(4) . 6_665
O29 Zn2 C56 25.1(4) 6_665 6_665
O11 Zn2 C56 100.7(4) . 6_665
N19 Zn2 C56 108.8(4) . 6_665
O30 Zn2 C56 134.0(4) . 6_665
O28 Zn2 C56 30.0(3) 6_665 6_665
N2 Zn3 N47 113.3(4) 6_665 5_665
N2 Zn3 O31 98.1(4) 6_665 .
N47 Zn3 O31 97.5(3) 5_665 .
N2 Zn3 O54 128.8(4) 6_665 .
N47 Zn3 O54 110.0(4) 5_665 .
O31 Zn3 O54 102.1(4) . .
N2 Zn3 O10 94.5(4) 6_665 .
N47 Zn3 O10 94.8(4) 5_665 .
O31 Zn3 O10 157.1(4) . .
O54 Zn3 O10 55.4(4) . .
N2 Zn3 C9 113.3(4) 6_665 .
N47 Zn3 C9 105.3(4) 5_665 .
O31 Zn3 C9 128.5(4) . .
O54 Zn3 C9 26.7(4) . .
O10 Zn3 C9 28.8(3) . .
Zn2 O30 Zn2 113.0(5) . 16_544
Zn2 O30 Zn1 107.6(3) . .
Zn2 O30 Zn1 107.6(3) 16_544 .
N3 N2 N1 110.7(8) . .
N3 N2 Zn3 129.8(8) . 7_645
N1 N2 Zn3 119.5(8) . 7_645
C2 N3 N2 107.1(8) . .
N2 N1 C1 108.6(8) . .
N2 N1 Zn1 120.7(7) . 10_644
C1 N1 Zn1 130.1(8) . 10_644
C5 C48 C4 120.8(10) . .
C5 C48 H48 119.6 . .
C4 C48 H48 119.6 . .
N3 C2 C1 110.4(9) . .
N3 C2 C4 123.8(11) . .
C1 C2 C4 125.8(11) . .
C58 C5 C48 118.6(10) . .
C58 C5 H5 120.7 . .
C48 C5 H5 120.7 . .
N1 C1 C2 103.3(9) . .
N1 C1 H1 128.4 . .
C2 C1 H1 128.4 . .
C7 C4 C48 120.6(10) . .
C7 C4 C2 115.6(10) . .
C48 C4 C2 123.3(10) . .
C56 O28 Zn2 78.7(8) . 7_645
C9 O10 Zn3 82.2(8) . .
C5 C58 C6 121.0(10) . .
C5 C58 C9 120.8(9) . .
C6 C58 C9 118.2(9) . .
O29 C56 O28 114.1(12) . .
O29 C56 C25 122.5(13) . .
O28 C56 C25 123.4(12) . .
O28 C56 Zn2 71.3(7) . 7_645
C25 C56 Zn2 165.3(9) . 7_645
C25 C55 C24 118.3(11) . .
C25 C55 H55 120.8 . .
C24 C55 H55 120.8 . .
C4 C7 C6 117.5(11) . .
C4 C7 H7 121.2 . .
C6 C7 H7 121.2 . .
C56 O29 Zn2 112.1(10) . 7_645
C55 C24 C23 122.2(11) . .
C55 C24 H24 118.9 . .
C23 C24 H24 118.9 . .
C55 C25 C26 122.5(11) . .
C55 C25 C56 118.3(11) . .
C26 C25 C56 119.2(10) . .
C58 C6 C7 121.4(11) . .
C58 C6 H6 119.3 . .
C7 C6 H6 119.3 . .
O54 C9 O10 123.8(13) . .
O54 C9 C58 119.9(12) . .
O10 C9 C58 116.3(11) . .
O54 C9 Zn3 55.0(7) . .
O10 C9 Zn3 69.0(7) . .
C58 C9 Zn3 172.9(9) . .
N19 C21 C22 108.0(10) . .
N19 C21 H21 126.0 . .
C22 C21 H21 126.0 . .
C24 C23 C57 117.6(11) . .
C24 C23 C22 114.0(10) . .
C57 C23 C22 127.7(11) . .
N20 N19 C21 109.0(10) . .
N20 N19 Zn2 120.0(8) . .
C21 N19 Zn2 130.4(8) . .
N18 C22 C23 127.1(11) . .
N18 C22 C21 102.5(9) . .
C23 C22 C21 130.3(11) . .
C25 C26 C57 117.6(11) . .
C25 C26 H26 121.2 . .
C57 C26 H26 121.2 . .
C9 O54 Zn3 98.3(10) . .
C26 C57 C23 121.8(11) . .
C26 C57 H57 119.1 . .
C23 C57 H57 119.1 . .
N19 N20 N18 108.9(9) . .
N19 N20 Zn1 121.9(8) . .
N18 N20 Zn1 128.7(8) . .
N20 N18 C22 111.2(9) . .
O11 C12 O11 116.6(15) . 16_544
O11 C12 C13 121.7(8) . .
O11 C12 C13 121.7(8) 16_544 .
C12 O11 Zn2 140.4(9) . .
C14 C13 C14 121.6(14) 16_544 .
C14 C13 C12 119.2(7) 16_544 .
C14 C13 C12 119.2(7) . .
C54 N47 N47 108.8(6) . 16_544
C54 N47 Zn3 133.0(7) . 5_664
N47 N47 Zn3 118.1(2) 16_544 5_664
N54 C16 C54 108.6(14) 16_544 .
C54 C16 C54 108.6(14) 16_544 .
N54 C16 C47 125.6(7) 16_544 .
C54 C16 C47 125.6(7) 16_544 .
C54 C16 C47 125.6(7) . .
C15 C47 C15 117.3(14) 16_544 .
C15 C47 C16 121.2(7) 16_544 .
C15 C47 C16 121.2(7) . .
C13 C14 C15 118.5(12) . .
C13 C14 H14 120.8 . .
C15 C14 H14 120.8 . .
N47 C54 C16 106.9(12) . .
N47 C54 H54 126.6 . .
C16 C54 H54 126.6 . .
C14 C15 C47 122.1(12) . .
C14 C15 H15 119.0 . .
C47 C15 H15 119.0 . .
Zn3 O31 Zn3 108.0(4) 16_544 .
Zn3 O31 Zn1 109.1(3) 16_544 .
Zn3 O31 Zn1 109.1(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 N1 2.093(8) 6_665
Zn1 N1 2.093(8) 10_654
Zn1 O31 2.177(8) .
Zn1 N20 2.180(9) 16_544
Zn1 N20 2.180(9) .
Zn1 O30 2.289(11) .
Zn2 O29 1.881(9) 6_665
Zn2 O11 1.932(8) .
Zn2 N19 1.936(10) .
Zn2 O30 1.966(6) .
Zn2 O28 2.477(10) 6_665
Zn2 C56 2.565(13) 6_665
Zn3 N2 1.969(9) 6_665
Zn3 N47 1.973(10) 5_665
Zn3 O31 1.992(5) .
Zn3 O54 2.109(10) .
Zn3 O10 2.400(11) .
Zn3 C9 2.547(11) .
O30 Zn2 1.966(6) 16_544
N2 N3 1.345(9) .
N2 N1 1.350(9) .
N2 Zn3 1.969(9) 7_645
N3 C2 1.325(10) .
N1 C1 1.384(13) .
N1 Zn1 2.093(8) 10_644
C48 C5 1.371(7) .
C48 C4 1.395(7) .
C48 H48 0.9500 .
C2 C1 1.434(11) .
C2 C4 1.445(8) .
C5 C58 1.367(7) .
C5 H5 0.9500 .
C1 H1 0.9500 .
C4 C7 1.381(7) .
O28 C56 1.308(12) .
O28 Zn2 2.477(10) 7_645
O10 C9 1.238(13) .
C58 C6 1.375(6) .
C58 C9 1.508(8) .
C56 O29 1.174(12) .
C56 C25 1.504(13) .
C56 Zn2 2.565(13) 7_645
C55 C25 1.367(7) .
C55 C24 1.374(7) .
C55 H55 0.9500 .
C7 C6 1.384(7) .
C7 H7 0.9500 .
O29 Zn2 1.881(9) 7_645
C24 C23 1.381(7) .
C24 H24 0.9500 .
C25 C26 1.378(7) .
C6 H6 0.9500 .
C9 O54 1.155(13) .
C21 N19 1.328(12) .
C21 C22 1.427(11) .
C21 H21 0.9500 .
C23 C57 1.391(7) .
C23 C22 1.419(7) .
N19 N20 1.303(10) .
C22 N18 1.350(11) .
C26 C57 1.388(7) .
C26 H26 0.9500 .
C57 H57 0.9500 .
N20 N18 1.317(10) .
C12 O11 1.196(9) .
C12 O11 1.196(9) 16_544
C12 C13 1.475(14) .
C13 C14 1.377(8) 16_544
C13 C14 1.377(8) .
N47 C54 1.296(11) .
N47 N47 1.365(14) 16_544
N47 Zn3 1.973(10) 5_664
C16 N54 1.356(11) 16_544
C16 C54 1.356(11) 16_544
C16 C54 1.356(11) .
C16 C47 1.476(9) .
C47 C15 1.386(8) 16_544
C47 C15 1.386(8) .
C14 C15 1.378(9) .
C14 H14 0.9500 .
C54 H54 0.9500 .
C15 H15 0.9500 .
O31 Zn3 1.992(5) 16_544
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.006 -0.022 0.007 19800 8032 ' '
